Using heavy-atom-containing xanthene dyes,benzoins can be quanti- tatively prepared by photosensitized reduction from benzils with triethyla- mine.It is an important supplement to'benzoin condensation',asp.for...Using heavy-atom-containing xanthene dyes,benzoins can be quanti- tatively prepared by photosensitized reduction from benzils with triethyla- mine.It is an important supplement to'benzoin condensation',asp.for those benzoins with electron-donating substituents.展开更多
Ni（HCO3）2 with unique phase and high crystallinity was synthesized with urea hydrolysis. The as-prepared samples were well characterized in detail. N2 adsorption and desorption result manifests a high surface area o...Ni（HCO3）2 with unique phase and high crystallinity was synthesized with urea hydrolysis. The as-prepared samples were well characterized in detail. N2 adsorption and desorption result manifests a high surface area of 99.03 m2/g with a pore size of 7.8 nm. Scanning electron microscopy （SEM） and particle size distribution reveal that the diameters of the formed pellets are uniform. Thermogravimetry （TG） analysis result shows that 500 ℃ could be the appropriate temperature for converting Ni（HCO3）2 precursors into NiO via a thermal decomposition process. CO2 and NH3 temperature-programmed desorption results show that Ni（HCO3）2 has explicit acid-base sites. Transmission electron microscopy （TEM） results vividly indicate that the pellets are aggregated by hexagonal platelets and possess porous structures. Ni（HCO3）2 can efficiently catalyze the one-step synthesis of benzoin ethyl ether from benzaldehyde and ethanol, with the conversion ofbenzaldehyde up to 57.5% and nearly 100% selectivity of benzoin ethyl ether.展开更多
The benzoin group caged compound has received strong interests due to its excellent photo- deprotection properties and wide use in chemical and biological studies. We used timeresolved infrared spectroscopy to investi...The benzoin group caged compound has received strong interests due to its excellent photo- deprotection properties and wide use in chemical and biological studies. We used timeresolved infrared spectroscopy to investigate the photochemical reaction of the benzoin caged compound, o-（2-methylbenzoyl）-DL-benzoin under 266 nm laser irradiation. Taking advantage of the specific vibrational marker bands and the IR discerning capability, we have detected and identified the uncaging product 2-methylbenzoic acid, and two intermediate radicals of benzoyl and 2-methylbenzoate benzyl in the transient infrared spectra. Our results provide spectral evidence to support the homolytic cleavage reaction of C-C=O bond in competition with the deprotection reaction. Moreover, the product yields of 2-methylbenzoic acid and benzoyl radical were observed to be affected by solvents and a largely water contalning solvent can be in favor of the deprotection reaction.展开更多
MgCoAl-hydrotalcite-like compounds （MgCoAI-HTLcs） were synthesized using the coprecipitation method of variable pH values. The effect of each factor on the preparation of HTLcs was discussed systematically, which in...MgCoAl-hydrotalcite-like compounds （MgCoAI-HTLcs） were synthesized using the coprecipitation method of variable pH values. The effect of each factor on the preparation of HTLcs was discussed systematically, which included pH values, mole ratios of Mg2＋ to Co2＋, the concentrations of the solution, and the temperature and time of the hydrothermal treatment. Besides, the thermal decomposition of MgCoAI-HTLcs was discussed. X-ray diffraction, thermogravimetric analysis, and FT-IR spectroscopy were performed to characterize the MgCoAI-HTLcs samples. The results showed that when the pH = 7.6-8.5 or 5.5-6.2, atomic ratios of （Mg^2＋＋Co2＋）/Al^3＋ 2 and Mg^2＋/Co^2＋ ranging from 1.00 to 2.00, temperature and time of hydrothermal treatment being 110℃ and 6 h, unique MgCoAI-HTLcs with high crystallinity could be obtained. When the calcination temperature was up to 250℃, the MgO phase was detected coexisting with Al2O3 and MgAl2O4 was highly spreaded on the derived mixed oxides. The synthesis reaction of benzoin methyl ether with methanol and benzaldehyde was chosen to study the catalytic activity of MgCoAI-HTLcs. The catalyst showed high activity and high stability in the synthesis of benzoin methyl ether in the feasible condition.展开更多
An efficient synthesis of benzoin isopropyl ether with benzaldehyde and propanol in the presence of heterogeneous recyclable Cu-Fe-hydrotalcite catalyst has been explored. Cu-Fe-hydrotalcite was firstly successfully s...An efficient synthesis of benzoin isopropyl ether with benzaldehyde and propanol in the presence of heterogeneous recyclable Cu-Fe-hydrotalcite catalyst has been explored. Cu-Fe-hydrotalcite was firstly successfully synthesized over Jahn-Teller effect of Cu^2＋. The catalytic test result showed that Cu-Fe-hydrotalcite could be used as a good catalyst in the synthesis of benzoin isopropyl ether. The highest conversion of ben- zaldehyde was 59.7% and the selectivity of benzoin isopropyl ether was nearly 100%. By this new method, not only was the cyanide poisoning avoided, but also the synthesis of benzoin isopropyl ether could be completed in one step instead of traditional two steps with both condensation and etherification.展开更多
A simple one-pot synthetic method for the preparation of 2,4,5-triaryl-lH-imidazoles from benzoin or benzil, ammonium acetate, aromatic aldehydes, and ZrOCl2-8H2O catalyst is described. The ZrOCl2-8H2O catalyst was fo...A simple one-pot synthetic method for the preparation of 2,4,5-triaryl-lH-imidazoles from benzoin or benzil, ammonium acetate, aromatic aldehydes, and ZrOCl2-8H2O catalyst is described. The ZrOCl2-8H2O catalyst was found to be equally effective for aromatic and heteroaromatic aldehydes and also for the preparation of substituted 1,4-di（4,5-diphenylimidazol-yl） benzene.展开更多
A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mi...A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mild reaction conditions to afford the corresponding trisubstituted imidazole in excellent yields.The method for synthesis of product,the reaction mixture was reflux in ethanol for 40-90 min.The present method is simple,efficient,and cost-effective.展开更多
Benzoin condensation promoted efficiently in three imidazolium based room tempera- ture ionic liquids [bmim]Br, [bmim]BF4 and [Bnmim]BF4 is reported for the first time. Benzoins were obtained in up to 91% yield within...Benzoin condensation promoted efficiently in three imidazolium based room tempera- ture ionic liquids [bmim]Br, [bmim]BF4 and [Bnmim]BF4 is reported for the first time. Benzoins were obtained in up to 91% yield within less than 30 min under mild conditions.展开更多
The oxygenation constants of transition-metal complexes with benzoin Schiff bases were measured and these complexes were first employed as models for mimicking monooxygenase in catalytic epoxidation of styrene. The hi...The oxygenation constants of transition-metal complexes with benzoin Schiff bases were measured and these complexes were first employed as models for mimicking monooxygenase in catalytic epoxidation of styrene. The highest conversion and selectivity were up to 39.6% and 100% respectively at ambient temperature and pressure. The effects of structures of the bridge group R in the ligands on the dioxygen affinities and catalytic activities to epoxidize styrene were also investigated.展开更多
A new mononuclear copper（Ⅱ） complex [（bipy）2Cu（PhCOO）]ClO4·（benzil） （bipy = 2,2＇-bipyridine, benzil = 1,2-diphenyl-ethane-1,2-dione） was synthesized by direct electrochemical oxidation of Cu electrode...A new mononuclear copper（Ⅱ） complex [（bipy）2Cu（PhCOO）]ClO4·（benzil） （bipy = 2,2＇-bipyridine, benzil = 1,2-diphenyl-ethane-1,2-dione） was synthesized by direct electrochemical oxidation of Cu electrode in an acetonitrile solution with benzoic acid, 2,2＇-bipyridine and benzoin. As soon as the current flowed in the cell, benzoin was oxidized to benzil quickly. The crystal structure was determined by X-ray diffraction. It belongs to monoclinic system, space group P21/c with a = 14.860（2）, b = 20.784（3）, c = 11.9150（17）A, β = 101.401（3）°, V= 3607.3（9）/k^3, Z = 4, M, = 806.69, D, = 1.485 g/cm^3, F（000） = 1660, μ = 0.742 mm^-1, R = 0.0788 and wR = 0.1519 for 6254 observed reflections （I 〉 2σ（I）. The complex contains a mononuclear [（bipy）2Cu（PhCOO）] cation, a solvate benzil molecule and a ClO4^- anion which locates around the cation outside acting as the counter ion. The Cu（ll） ion is coordinated by two 2,2＇-bipyridines and one benzoato ligand to form a distorted square-pyramid.展开更多
Schiff base was synthesized by using salicylaldehyde and ethylenediamine as raw materials,and then Co(Salen)complex was synthesized by using Schiff base and Co.The structure and purity of the samples were tested by ma...Schiff base was synthesized by using salicylaldehyde and ethylenediamine as raw materials,and then Co(Salen)complex was synthesized by using Schiff base and Co.The structure and purity of the samples were tested by mass spectrum.Then the orthogonal test method was used to study the catalytic performance of the complex in the reaction of benzil produced from benzoin,and the optimal reaction conditions were obtained finally.The results showed when the reaction temperature was 80℃,and the reaction time was 2h,the yield of benzil produced from benzoin by using Co(Salen)as catalyst reached the maximum 37.28%.展开更多
The chemical cellular signaling pathway of phosphatidylinositol-3-kinase(PI3K)is crucial in many aspects of cell growth and survival.Genetic alterations such as amplification,mutation and chromosomal transposition can...The chemical cellular signaling pathway of phosphatidylinositol-3-kinase(PI3K)is crucial in many aspects of cell growth and survival.Genetic alterations such as amplification,mutation and chromosomal transposition can compromise the PI3K pathway,leading to its permanent activation,which results in the alteration of growth control and cell survival mechanisms,favoring competitive growth,metastatic capacity,and often a greater resistance to treatments.Evidence of these destructive genetic modifications has been found in different types of cancer.Recently,a group of researchers found that the structure of benzoin matches the fingerprint of the active PI3K inhibitor.The focus of this work is on the synthesis of substituted benzoins via benzoin condensation in aqueous medium for subsequent reaction with anilines.The aim is to obtain a series of new compounds derived from 1,2-diphenyliminoethanol,which will be sent to a specialized laboratory to evaluate their cytotoxicity on carcinoma cell lines.展开更多
Two novel monobenzo porphyrazines bearing nitro and methoxyl respectively on fused benzene ring were suc- cessfully synthesized. Also, an asymmetrical porphyrazine with one butylthio branch at the pyrrolic p-position ...Two novel monobenzo porphyrazines bearing nitro and methoxyl respectively on fused benzene ring were suc- cessfully synthesized. Also, an asymmetrical porphyrazine with one butylthio branch at the pyrrolic p-position sub- stituted by hydrogen atom was successfully isolated in the course of synthesis of symmetric octakis（butylthio） porphyrazine. Their corresponding cobalt complexes were subsequently obtained and characterized. Their catalytic ability was assessed by aerobic oxidation of benzoin, showing the highest benzil yield of 95.2% for 60 min. A pos- sible mechanism was also presented from the in-situ UV-Vis spectra, in which a novel and characteristic absorption peak of metal-oxo was observed. At the same time, similar results of the extended oxidation of benzyl alcohol also confirmed the reactive mechanism.展开更多
文摘Using heavy-atom-containing xanthene dyes,benzoins can be quanti- tatively prepared by photosensitized reduction from benzils with triethyla- mine.It is an important supplement to'benzoin condensation',asp.for those benzoins with electron-donating substituents.
基金Project(50872086)supported by the National Natural Science Foundation of ChinaProject(2012021006-3)supported by the Natural Science Foundation of Shanxi Province,China+1 种基金Project(2012L022)supported by Special/Youth Foundation of Taiyuan University of Technology,ChinaProject(20120321033-02)supported by Science and Technology Research of Shanxi Province,China
文摘Ni（HCO3）2 with unique phase and high crystallinity was synthesized with urea hydrolysis. The as-prepared samples were well characterized in detail. N2 adsorption and desorption result manifests a high surface area of 99.03 m2/g with a pore size of 7.8 nm. Scanning electron microscopy （SEM） and particle size distribution reveal that the diameters of the formed pellets are uniform. Thermogravimetry （TG） analysis result shows that 500 ℃ could be the appropriate temperature for converting Ni（HCO3）2 precursors into NiO via a thermal decomposition process. CO2 and NH3 temperature-programmed desorption results show that Ni（HCO3）2 has explicit acid-base sites. Transmission electron microscopy （TEM） results vividly indicate that the pellets are aggregated by hexagonal platelets and possess porous structures. Ni（HCO3）2 can efficiently catalyze the one-step synthesis of benzoin ethyl ether from benzaldehyde and ethanol, with the conversion ofbenzaldehyde up to 57.5% and nearly 100% selectivity of benzoin ethyl ether.
基金This work was supported by the National Natural Science Foundation of China （No.21333012 and No.21425313） and the National Basic Research Program of China （No.2013CB834602）.
文摘The benzoin group caged compound has received strong interests due to its excellent photo- deprotection properties and wide use in chemical and biological studies. We used timeresolved infrared spectroscopy to investigate the photochemical reaction of the benzoin caged compound, o-（2-methylbenzoyl）-DL-benzoin under 266 nm laser irradiation. Taking advantage of the specific vibrational marker bands and the IR discerning capability, we have detected and identified the uncaging product 2-methylbenzoic acid, and two intermediate radicals of benzoyl and 2-methylbenzoate benzyl in the transient infrared spectra. Our results provide spectral evidence to support the homolytic cleavage reaction of C-C=O bond in competition with the deprotection reaction. Moreover, the product yields of 2-methylbenzoic acid and benzoyl radical were observed to be affected by solvents and a largely water contalning solvent can be in favor of the deprotection reaction.
基金Supported by the Natural Science Foundation of Shanxi Province(20001015).
文摘MgCoAl-hydrotalcite-like compounds （MgCoAI-HTLcs） were synthesized using the coprecipitation method of variable pH values. The effect of each factor on the preparation of HTLcs was discussed systematically, which included pH values, mole ratios of Mg2＋ to Co2＋, the concentrations of the solution, and the temperature and time of the hydrothermal treatment. Besides, the thermal decomposition of MgCoAI-HTLcs was discussed. X-ray diffraction, thermogravimetric analysis, and FT-IR spectroscopy were performed to characterize the MgCoAI-HTLcs samples. The results showed that when the pH = 7.6-8.5 or 5.5-6.2, atomic ratios of （Mg^2＋＋Co2＋）/Al^3＋ 2 and Mg^2＋/Co^2＋ ranging from 1.00 to 2.00, temperature and time of hydrothermal treatment being 110℃ and 6 h, unique MgCoAI-HTLcs with high crystallinity could be obtained. When the calcination temperature was up to 250℃, the MgO phase was detected coexisting with Al2O3 and MgAl2O4 was highly spreaded on the derived mixed oxides. The synthesis reaction of benzoin methyl ether with methanol and benzaldehyde was chosen to study the catalytic activity of MgCoAI-HTLcs. The catalyst showed high activity and high stability in the synthesis of benzoin methyl ether in the feasible condition.
基金support from the National Natural Science Foundation of China (50872086)the Natural Science Foundation of Shanxi Province(2008011018)
文摘An efficient synthesis of benzoin isopropyl ether with benzaldehyde and propanol in the presence of heterogeneous recyclable Cu-Fe-hydrotalcite catalyst has been explored. Cu-Fe-hydrotalcite was firstly successfully synthesized over Jahn-Teller effect of Cu^2＋. The catalytic test result showed that Cu-Fe-hydrotalcite could be used as a good catalyst in the synthesis of benzoin isopropyl ether. The highest conversion of ben- zaldehyde was 59.7% and the selectivity of benzoin isopropyl ether was nearly 100%. By this new method, not only was the cyanide poisoning avoided, but also the synthesis of benzoin isopropyl ether could be completed in one step instead of traditional two steps with both condensation and etherification.
文摘A simple one-pot synthetic method for the preparation of 2,4,5-triaryl-lH-imidazoles from benzoin or benzil, ammonium acetate, aromatic aldehydes, and ZrOCl2-8H2O catalyst is described. The ZrOCl2-8H2O catalyst was found to be equally effective for aromatic and heteroaromatic aldehydes and also for the preparation of substituted 1,4-di（4,5-diphenylimidazol-yl） benzene.
文摘A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mild reaction conditions to afford the corresponding trisubstituted imidazole in excellent yields.The method for synthesis of product,the reaction mixture was reflux in ethanol for 40-90 min.The present method is simple,efficient,and cost-effective.
基金We thank the financial support from the National Natural Science Foundation of China.(No.20172038)
文摘Benzoin condensation promoted efficiently in three imidazolium based room tempera- ture ionic liquids [bmim]Br, [bmim]BF4 and [Bnmim]BF4 is reported for the first time. Benzoins were obtained in up to 91% yield within less than 30 min under mild conditions.
文摘The oxygenation constants of transition-metal complexes with benzoin Schiff bases were measured and these complexes were first employed as models for mimicking monooxygenase in catalytic epoxidation of styrene. The highest conversion and selectivity were up to 39.6% and 100% respectively at ambient temperature and pressure. The effects of structures of the bridge group R in the ligands on the dioxygen affinities and catalytic activities to epoxidize styrene were also investigated.
基金This work was supported by the National Natural Science Foundation of China (No. 20503019)
文摘A new mononuclear copper（Ⅱ） complex [（bipy）2Cu（PhCOO）]ClO4·（benzil） （bipy = 2,2＇-bipyridine, benzil = 1,2-diphenyl-ethane-1,2-dione） was synthesized by direct electrochemical oxidation of Cu electrode in an acetonitrile solution with benzoic acid, 2,2＇-bipyridine and benzoin. As soon as the current flowed in the cell, benzoin was oxidized to benzil quickly. The crystal structure was determined by X-ray diffraction. It belongs to monoclinic system, space group P21/c with a = 14.860（2）, b = 20.784（3）, c = 11.9150（17）A, β = 101.401（3）°, V= 3607.3（9）/k^3, Z = 4, M, = 806.69, D, = 1.485 g/cm^3, F（000） = 1660, μ = 0.742 mm^-1, R = 0.0788 and wR = 0.1519 for 6254 observed reflections （I 〉 2σ（I）. The complex contains a mononuclear [（bipy）2Cu（PhCOO）] cation, a solvate benzil molecule and a ClO4^- anion which locates around the cation outside acting as the counter ion. The Cu（ll） ion is coordinated by two 2,2＇-bipyridines and one benzoato ligand to form a distorted square-pyramid.
文摘Schiff base was synthesized by using salicylaldehyde and ethylenediamine as raw materials,and then Co(Salen)complex was synthesized by using Schiff base and Co.The structure and purity of the samples were tested by mass spectrum.Then the orthogonal test method was used to study the catalytic performance of the complex in the reaction of benzil produced from benzoin,and the optimal reaction conditions were obtained finally.The results showed when the reaction temperature was 80℃,and the reaction time was 2h,the yield of benzil produced from benzoin by using Co(Salen)as catalyst reached the maximum 37.28%.
文摘The chemical cellular signaling pathway of phosphatidylinositol-3-kinase(PI3K)is crucial in many aspects of cell growth and survival.Genetic alterations such as amplification,mutation and chromosomal transposition can compromise the PI3K pathway,leading to its permanent activation,which results in the alteration of growth control and cell survival mechanisms,favoring competitive growth,metastatic capacity,and often a greater resistance to treatments.Evidence of these destructive genetic modifications has been found in different types of cancer.Recently,a group of researchers found that the structure of benzoin matches the fingerprint of the active PI3K inhibitor.The focus of this work is on the synthesis of substituted benzoins via benzoin condensation in aqueous medium for subsequent reaction with anilines.The aim is to obtain a series of new compounds derived from 1,2-diphenyliminoethanol,which will be sent to a specialized laboratory to evaluate their cytotoxicity on carcinoma cell lines.
基金This work was financially supported by National Natural Science Foundation of China （Nos. 20977115 and 21272281）, Natural Science Foundation of Hubei Province （No. 2014CFB919） and the S＆T Plan Innovation team of Wuhan city （No. 2015070504020220）.
文摘Two novel monobenzo porphyrazines bearing nitro and methoxyl respectively on fused benzene ring were suc- cessfully synthesized. Also, an asymmetrical porphyrazine with one butylthio branch at the pyrrolic p-position sub- stituted by hydrogen atom was successfully isolated in the course of synthesis of symmetric octakis（butylthio） porphyrazine. Their corresponding cobalt complexes were subsequently obtained and characterized. Their catalytic ability was assessed by aerobic oxidation of benzoin, showing the highest benzil yield of 95.2% for 60 min. A pos- sible mechanism was also presented from the in-situ UV-Vis spectra, in which a novel and characteristic absorption peak of metal-oxo was observed. At the same time, similar results of the extended oxidation of benzyl alcohol also confirmed the reactive mechanism.
